関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 反応物 | 3,3-Bis-(4-pyridin-3-yl-phenyl)-prop-2-en-1-ol | HCID 21986819 | — |
| 反応物 | Ethyl [4-sulfanyl-2-(trifluoromethyl)phenoxy]acetate | HCID 59516001 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | {4-[3,3-Bis-(4-pyridin-3-yl-phenyl)-allylsulfanyl]-2-trifluoromethyl-phenoxy}-acetic acid ethyl ester | HCID 69620630 | — |
反応手順
Triphenylphosphine (138 mg, 0.68 mmol) and ADDP (173 mg, 0.68 mmol) were added to a solution of 3,3-bis-(4-pyridin-3-yl-phenyl)-prop-2-en-1-ol (100 mg, 0.27 mmol) in THF (5 ml) at 0° C. The reaction mixture was stirred for 5 min under nitrogen atmosphere. (4-Mercapto-2-trifluoromethyl-phenoxy)-acetic acid ethyl ester (prepared analogous to procedure in BioOrg. Med. Chem. Lett. 2003, 13, 1517) (92 mg, 0.32 mmol) was slowly added to the reaction mixture and the reaction was stirred for further 2 h at 0° C. The reaction mixture was evaporated and the residue was triturated with ether (2×15 ml). The filtered ether phases were evaporated and purified by column chromatography (eluent: ethyl acetate) to give {4-[3,3-bis-(4-pyridin-3-yl-phenyl)-allylsulfanyl]-2-trifluoromethyl-phenoxy}-acetic acid ethyl ester in 100 mg (60%) yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091245B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-c5ebe0b0aed846cc89d4466e7663f9a1 |
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| 出典メモ | uspto-grants-2006_08 |
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